CN1128850C - Rigid painted polyurea material and its construction method - Google Patents
Rigid painted polyurea material and its construction method Download PDFInfo
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- CN1128850C CN1128850C CN 01114995 CN01114995A CN1128850C CN 1128850 C CN1128850 C CN 1128850C CN 01114995 CN01114995 CN 01114995 CN 01114995 A CN01114995 A CN 01114995A CN 1128850 C CN1128850 C CN 1128850C
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Abstract
The present invention discloses a spray type rigid polyurea material with the solid content of 100 % and a construction method thereof. The material is composed of a component A and a component R, wherein the component A is a semi-prepolymer synthesized by 65 to 75 portions of polyisocyanate and 25 to 35 portions of polyether polyol; the component R comprises 5 to 30 portions of chain extender, 40 to 60 portions of terminal amino group polyether and 10 to 30 portions of flame retardant. When the material is sprayed on a foamed base material, a tough protective layer is instantly formed. The present invention is mainly applied to the fields of film properties and scenes, decorative materials, sculptures, specimen, display plates for exhibition, etc.
Description
Technical field
The present invention relates to a kind of flame retardant type rigid painted polyurea material, specifically is the flame retardant type rigid painted polyurea material that is applied in the foam protection, and constructional method.
Background technology
In industries such as video display, theater, advertisement, theme park, building decorations, polystyrene foam (EPS), polyurethane foam materials such as (PUF) are used to make moulding products such as the stage property, setting, sculpture of different shapes,, craft in light weight because of them or computer sculpture easy row easy to process are the materials that a kind of ideal is made various moulding.But be to use big defective of foamy to be: surface durability is relatively poor, many in some moulding quantity, volume is big, and need be as the occasion of outdoor exhibition, exist such as many hidden danger of damaging of causing such as bump, wearing and tearing, also therefore brought a large amount of financial losses.For addressing this problem, need protect meticulous finished foam moulding outside surface with all good light materials of a kind of shock-resistance, wear resistance, weathering resistance and workability.Spraying rigidity polyurea materials is simple because of its construction, performance foam original shape, can be used as a good solution.
A kind of spraying rigid polyurethane material is disclosed in United States Patent (USP) 4940558 the insides, it is 100 parts of many phenyl polymethine polyisocyanates of 32.1% that this patent A component adopts the end isocyano, and it is that 250 21.8 parts of hydroxy polyethers trivalent alcohols, hydroxyl value are that 28 49.2 parts of hydroxy polyethers dibasic alcohol, hydroxyl value are that 770 13.1 parts of hydroxy polyethers tetravalent alcohols, hydroxyl value are formations such as 1810 15.8 parts of dibasic alcohol chainextenders, 0.1 part of dibutyl tin laurate that the B component adopts hydroxyl value.The volume ratio of A, B component is 1: 1, adopts polycomponent high pressure painting equipment to construct.Its performance is that tensile strength is 21～63Mpa, and elongation at break is 5～100%, and modulus in flexure is 350～3150Mpa, and hardness is Shao Shi D30～80, and density is 0.3～2.4Kg/m
3, can be used to make artificial rock true to nature in dry season, but this polyurethane material is higher than at 85% o'clock in humidity, tangible foamed phenomenon is just arranged and wait in the winter time under the lower situation of temperature, set time is long, and problems such as trickling are arranged.
In United States Patent (USP) 5962618, the Dudley J Primeaux II of U.S. Huntsman company discloses a kind of spray polyurea elastomer material that is used for the wagon box wear resistance lining.The A component is a semi-prepolymer in the prescription of this patent, by at least 50% 2,4 '-diphenylmethanediisocyanate and 4, the mixture of 4 '-diphenylmethanediisocyanate and polyether glycol are synthetic, and wherein diphenylmethanediisocyanate (MDI) accounts for 35～65 parts.The B component is the mixture that 0.3～0.8 part of functional epoxy silane, 0.2～0.3 part in water etc. such as 25～40 parts of 55～45 parts of Jeffamine Amino Terminated polyether(ATPE)s, amine chain extender, the Silquest 187 of Huntsman company constitute.The volume ratio of A, B component is 1: 1, adopts polycomponent high pressure painting equipment to construct.Performance is: tensile strength is 15Mpa, elongation at break be 520%, 300% modulus be 10.1Mpa, hardness be Shao Shi D43, can be used for through the carbon steel ground of shop primer, play a part wear-resisting, attractive in appearance, easy to clean.Though this material has solved moisture foaming, low-temperature curing and waited a difficult problem slowly, belongs to resilient material, in the application of foam protection, be difficult to reach the rigidity requirement.And rigid painted polyurea material is not seen any patent disclosure.
Summary of the invention
The purpose of this invention is to provide a kind of flame retardant type rigid painted polyurea material of moisture, temperature effect that is not subjected to and replace traditional spraying polyurethane rigid material.
Flame retardant type rigid painted polyurea material of the present invention comprises two kinds of components of A, R, and wherein the A component is the polyether glycol synthetic semi prepolymer by 65～75 parts of (unless following specified otherwise is parts by weight) polyisocyanates and 25～35 parts; The R component comprises 5～30 parts of chainextenders, 40～60 parts of Amino Terminated polyether(ATPE)s, 10～30 parts of fire retardants.
Said polyether glycol can be selected from polyglycol ether, polypropylene glycol ether, polyglycerol ether, polypentaerythritol ether, PTMG and above-mentioned one or more multipolymer, chooses wherein one or more; Also can be selected from the polyether glycol of low-unsaturation-degree, for example the TDB-2000 of Plant of Tianjin Petrochemical Company three factories.The hydroxyl equivalent of polyether glycol is higher than 500, and its functionality is between 2 to 4.
It is ethylene oxide-capped more than 22% that described polyether glycol is preferably.
Said polyisocyanates can be selected from 4 of carbodiimide-uretonimine-modified, 4 '-diphenylmethanediisocyanate, 4,4 '-diphenylmethanediisocyanate, 2,4 '-diphenylmethanediisocyanate, the many phenyl isocyanate of polymethine, choose wherein one or more, its functionality is higher than 2.0, and preferably 2.0～2.7.
The synthetic method of said A component is: the polyisocyanates of accurate measurement is joined in the reactor of nitrogen protection; at the uniform velocity stir; be heated to 50～80 ℃; the polyether glycol that in reactor, slowly adds metering; under 60～90 ℃, insulation reaction three hours, sampling analysis; survey free isocyanate group (NCO) content in the gained semi prepolymer between 18～25%, cooling discharging.
Chainextender in the said R component comprises: amine chain extender, for example: diethyl toluene diamine (DETDA), diformazan sulfenyl tolylene diamine (DMTDA), N, N ' two sec-butyl methylene dianiline (MDA)s, 4,4 '-diaminodiphenyl-methane, 3,3 '-two chloro-4,4 '-diaminodiphenyl-methane, aliphatic polyamine are chosen wherein one or more; Also can use the alcohols chainextender, for example: 1,4-butyleneglycol, 1,3 butylene glycol, TriMethylolPropane(TMP), glycerol, trolamine are chosen wherein one or more; Also can use the mixture of amine chain extender and alcohols chainextender.Its functionality is most typical to be between 2 to 3.
Amino Terminated polyether(ATPE) in the R component can be selected the JEFFAMINE of Huntsman company for use
D-2000, T-3000, D-4000 or T-5000 etc.
Fire retardant in the R component is an employed fire retardant in the common polyurethane system, comprises phosphoric acid ester, for example dimethyl methyl orthophosphoric acid, 3-β-chloropropyl phosphoric acid ester, 3-dichloro propyl phosphate; Bromated compound, for example dibromo phenyl polyvalent alcohol, tribromo phenyl alcohol also can add aluminium hydroxide, zinc borate, antimonous oxide etc.
In the R component, also can add stabilization aids such as oxidation inhibitor, ultraviolet absorbers as required.For example use the IRGANOX 1010 and the oxidation inhibitor such as 1076 of CIBA GEIGY company, and TINUVIN P, 327, ultraviolet absorbers such as 328, the consumption of this analog assistant is 0.3～2 part.
In the R component, also can add color stuffing as required.For example glass, carbon black, lime carbonate, talcum powder, kaolin, zeolite, diatomite, barium sulfate, perlite, vermiculite, titanium dioxide, the consumption of color stuffing is 5～30 parts.
The preparation method of R component is:
(1) if add color stuffing, then at first the Amino Terminated polyether(ATPE) in color stuffing and the part R component is made mixture, be dispersed into mill base with grinding plant such as sand mills then.According to prescription ground mill base, remainder Amino Terminated polyether(ATPE), chainextender, fire retardant are joined in the system paint can at last, utilize high-shear dispersing apparatus high-speed stirring to make in 30 minutes.
(2) if do not add color stuffing,, usefulness high-shear dispersing apparatus high-speed stirring such as Amino Terminated polyether(ATPE), chainextender, fire retardant were made in 30 minutes then according to formula ratio.
The equivalence ratio of A, R component, just isocyanate index is between 0.9～1.2.
The constructional method of the fire-retardant polyureas rigid material of the present invention is: after two components of A, R are measured, pressurize, heated up in the high pressure painting equipment of 1: 1 fixed volume ratio, be sprayed onto on the ground by spray gun, solidify the flame retardant type rigid painted polyurea material.The initial temperature of A, R material is higher than 10 ℃, and setting main frame pressure is 55～70Kg/cm
2, temperature is 50～60 ℃, the spray pressure difference of two components is lower than 14Kg/cm in the spray gun mixing section
2
Flame retardant type rigid painted polyurea material of the present invention, stable performance, heat release relax, and are not subjected to humidity, Temperature Influence, and curing speed is fast, generally is lower than in time of 15 seconds promptly curable.Traditional polyurea elastomer material mechanism is thought: the functionality of polyisocyanates is high more, the over-all properties of the final material that forms is poor more, this is because highly active Amino Terminated polyether(ATPE) at first reacts with highly active polyisocyanates, partial reaction is finished rapidly, and transfer reaction is not carried out.After the curing, the whole mechanics poor-performing of material.The present invention acts in a diametrically opposite way, and adopts the polyisocyanates of high functionality synthesize semi-prepolymer in the A component, solidifies the rigidity coating of back formation one deck hardness height, homogeneous thickness that toughness is strong, and this coating has shown excellent comprehensive mechanical properties.In the present invention, the A component can adopt the polyether glycol of low-unsaturation-degree, because of its reactive behavior is lower, has not only effectively alleviated the heat release of polyureas formation reaction, and because of its narrow molecular weight distribution, makes the toughness of material of final formation good; By suitable adjustment isocyanate index, can the optimization better comprehensive mechanical property, also can further improve its low-temperature impact resistance by suitably introducing the alcohols chainextender.Foams such as this coating and EPS, PUF are used, and are applied to movie prop, setting, building and ornament materials, theme park, sculpture, sample and advertisement with fields such as boards.Again because this material antiseptic performance is good, and for example its 1 millimeter coating salt spray resistance is 5000 hours, reaches one-level, so at sea in the metal heavy-duties such as oil drilling platform, underground tank, oil and gas pipelines, this coating has also shown excellent performance.
Compare with traditional spraying polyurethane rigid material, superiority of the present invention shows: (1) is not subjected to the influence of temperature, humidity; (2) stable performance; (3) can obtain different appearance effect, for example orange peel shape, smooth shape etc. by the conversion prescription; (4) alleviate exothermic heat of reaction, solved polystyrene foam produces gross distortion because of heat release in the absorbing sets problem.
By following examples as can be seen; rigid painted polyurea material of the present invention not only is not subjected to the influence of temperature, humidity; and performance satisfied the needs of foam protection with rigid material fully, reached flame retardant effect simultaneously, thereby can be applied to many fields safely, effectively.
Embodiment
Below provide several exemplary embodiments, but the present invention is confined to not merely in the following example.
The performance index introduction of following examples:
(1) condition of surface observation, gel time, sticking time all are to record on the ground at expanded polystyrene (EPS).
(2) salt spray resistance model preparation: at first being of a size of 80 * 140 millimeters, the carbon steel model sandblasting of 2 mm thick sprays 1 millimeter coating then immediately and makes to the Sa2.5 level.
(3) all the other performance index preparation of specimen: at first scribbling spraying one deck uniform coating on the sheet glass of releasing agent, the demoulding after 10 minutes requires to make according to sample preparation then.
Embodiment 1:
The preparation of A component: with 58.5 parts of MDI-100 (Yantai Synthetic Leather Factory), 23.4 parts of Isonate
143L (U.S. DOW company) polyisocyanates joins in the reactor of nitrogen protection; at the uniform velocity stir; be warmed up to 60 ℃; 32.4 parts of hydroxyl equivalents of slow adding are 1000 low-unsaturation-degree polyether dibasic alcohol (Plant of Tianjin Petrochemical Company three factories) in reactor; under 60～90 ℃, insulation reaction three hours, sampling analysis; etc. free isocyano-content stable after, i.e. cooling discharging.After the analysis free isocyano-content (NCO%) is 22% semi prepolymer.
The preparation of R component: earlier 5 parts of titanium dioxides and 5 parts of JEFFAMINE D-2000 are mixed with High shear device, with sand mill this mixture is made particle diameter less than 50 microns mill base then.
35 parts of JEFFAMINE D-2000,25 parts of DETDA, 20 parts of DMTDA, 5 part 1,4 butyleneglycols, 10 parts of titanium white mill bases, 10 parts of dimethyl methyl orthophosphoric acids, 1 part of Irganox1076 and 1 part of Tinuvin 328 join in the system paint can, use high-shear dispersing apparatus high-speed stirring 30 minutes.
The isocyanate index of this system is 1.14.
Constructional method: A, R component were preheating to 20 ℃ respectively before using, use the H-3500 main frame of U.S. Gusmer company and GX-7 spray gun to spray by 1: 1 (volume ratio), main frame pressure is set at 60Kg/cm
2, the main heating of A, R component and pipe Heating temperature are set at 55 ℃, and spraying dynamic pressure A component is 140Kg/cm
2, the R component is 142Kg/cm
2, envrionment temperature: 0 ℃, ambient moisture: 40%.The polyureas rigid material performance index of spraying gained are listed in the table below:
Gel time/second 3
Sticking time/minutes 30
Modulus in flexure/MPa 1400
Tensile strength MPa 45
Elongation at break/% 30
Density Kg/m
31.09
Surface hardness/Shao D 70
Cantilever beam impact strength 650
/m/kg/cm
Appearance state orange peel shape
Salt spray resistance (1mm coating, 1 grade
5000 hours)
Oxygen index 26
Embodiment 2:
The preparation of A component: with 58.4 parts of MDI-100,23.2 parts of PM-300 (Yantai Synthetic Leather Factory) and 33.3 parts of hydroxyl equivalents is 1000 polyether-tribasic alcohol (551C, the big chemistry in east), synthetic that NCO% is 20% semi prepolymer by the technology of embodiment 1.
The preparation of R component: identical with embodiment 1.
The isocyanate index of this embodiment is 1.03.
Constructional method: envrionment temperature: 32 ℃, ambient moisture: 95%.All the other are identical with embodiment 1.The performance index that spraying forms the polyureas rigid material are:
Gel time/second 10
Sticking time/minutes 25
Modulus in flexure/Mpa 1760
Tensile strength Mpa 45
Elongation at break/% 6
Density Kg/m
31.10
Surface hardness/Shao D 71
Cantilever beam impact strength 512
/m/kg/cm
The appearance state is smooth
Salt spray resistance (1mm coating, 1 grade
5000 hours)
Oxygen index 26
Embodiment 3:
The preparation of A component: according to the synthetic method of embodiment 1 with Isonate
89.7 parts of 143L and hydroxyl equivalent are that 25.3 parts of 1000 polyether Glycols (Tdiol-2000, Plant of Tianjin Petrochemical Company three factories) are synthetic that NCO% is 20% semi prepolymer.
The preparation of R component: identical with embodiment 1.
The isocyanate index of this embodiment is 1.03.
Constructional method: identical with embodiment 1.The performance index that spraying forms the polyureas rigid material are:
Gel time/second 3
Sticking time/minutes 30
Modulus in flexure/Mpa 1430
Tensile strength Mpa 40
Elongation at break/% 8
Surface hardness/Shao D 71
Density Kg/m
31.09
Cantilever beam impact strength 532
/m/kg/cm
The appearance state is smooth
1 grade of salt spray resistance
The 1mm coating, 5000 hours
Oxygen index 26
Embodiment 4:
The preparation of A component: with embodiment 1.
The preparation of R component: 40 parts of JEFFAMINED-2000,25 parts of DETDA, 25 parts of DMTDA, 15 parts of 3-β-chloropropyl phosphoric acid ester are made mixture in the system paint can, high-speed stirring made in 30 minutes on the high-shear dispersing apparatus.
Isocyanate index is 1.18
Constructional method: with embodiment 2.
Gel time/second 3
Sticking time/minutes 30
Modulus in flexure/MPa 1510
Tensile strength MPa 54
Elongation at break/% 2
Density Kg/m
31.09
Surface hardness/Shao D 70
Cantilever beam impact strength 442
/m/kg/cm
Appearance state orange peel shape
1 grade of salt spray resistance
The 1mm coating, 5000 hours
Oxygen index 27
Claims (10)
1, a kind of flame retardant type rigid painted polyurea material is characterized in that: be made up of A, R two components, by weight, the A component is by 65～75 parts of polyisocyanates and 25～35 parts of polyether glycol synthetic semi prepolymers; The R component comprises 5～30 parts of chainextenders, 40～60 parts of Amino Terminated polyether(ATPE)s, 10～30 parts of fire retardants.
2, according to the flame retardant type rigid painted polyurea material of claim 1, it is characterized in that: the isocyanate index of this material is between 0.9～1.2.
3, according to the flame retardant type rigid painted polyurea material of claim 1; it is characterized in that: the synthetic method of A component: the polyisocyanates adding of accurate measurement is had in the reactor of nitrogen protection; at the uniform velocity stir; be heated to 50-80 ℃, in reactor, slowly add the polyether glycol of accurate measurement, under 60～90 ℃; insulation reaction 3 hours; sampling analysis is surveyed free isocyanate group (NCO) content in the gained semi prepolymer between 18～25%, cooling discharging.
4, according to the flame retardant type rigid painted polyurea material of claim 1, it is characterized in that: described polyisocyanates is selected from 4 of carbodiimide-uretonimine-modified, 4 '-diphenylmethanediisocyanate, 4,4 '-diphenylmethanediisocyanate, 2,4 '-diphenylmethanediisocyanate, the many phenyl isocyanate of polymethine, choose wherein one or more, its functionality is higher than 2.0.
5, according to the flame retardant type rigid painted polyurea material of claim 4, it is characterized in that: the functionality of described polyisocyanates is 2.0～2.7.
6, according to the flame retardant type rigid painted polyurea material of claim 1, it is characterized in that: described polyether glycol is to be selected from polyglycol ether, polypropylene glycol ether, polyglycerol ether, polypentaerythritol ether, PTMG and above-mentioned one or more multipolymer, chooses wherein one or more; Also can be selected from the polyether glycol of low-unsaturation-degree; The functionality of polyether glycol is 2～4, and hydroxyl equivalent is at least more than 500.
7, according to the flame retardant type rigid painted polyurea material of claim 6, it is characterized in that: described polyether glycol is ethylene oxide-capped more than 22%.
8, according to the flame retardant type rigid painted polyurea material of claim 1, it is characterized in that: the chainextender in the R component comprises amine chain extender: diethyl toluene diamine, diformazan sulfenyl tolylene diamine, N, N ' two sec-butyl methylene dianiline (MDA)s, 4,4 '-diaminodiphenyl-methane, 3,3 '-two chloro-4,4 '-diaminodiphenyl-methane, aliphatic polyamine are chosen wherein one or more; Also comprise the alcohols chainextender: 1,4-butyleneglycol, 1,3 butylene glycol, TriMethylolPropane(TMP), glycerol, trolamine are chosen wherein one or more; Also can use the mixture of amine chain extender and alcohols chainextender; Its functionality is between 2 to 3.
9, according to the flame retardant type rigid painted polyurea material of claim 1, it is characterized in that: the fire retardant in the R component is selected from dimethyl methyl orthophosphoric acid, 3-β-chloropropyl phosphoric acid ester, 3-dichloro propyl phosphate, dibromo phenyl polyvalent alcohol, tribromo phenyl alcohol, also can add aluminium hydroxide, zinc borate, antimonous oxide, choose wherein one or more.
10, according to the flame retardant type rigid painted polyurea material of claim 1, it is characterized in that: also can add oxidation inhibitor, ultraviolet absorbers or color stuffing in the R component.
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| CN 01114995 CN1128850C (en) | 2001-05-30 | 2001-05-30 | Rigid painted polyurea material and its construction method |
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| CN 01114995 CN1128850C (en) | 2001-05-30 | 2001-05-30 | Rigid painted polyurea material and its construction method |
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| CN1128850C true CN1128850C (en) | 2003-11-26 |
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| CN 01114995 Expired - Fee Related CN1128850C (en) | 2001-05-30 | 2001-05-30 | Rigid painted polyurea material and its construction method |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037587B (en) * | 2007-04-03 | 2010-11-10 | 山东斯泰普力高新建材有限公司 | Polyurea elastomer construction engineering waterproof material |
| US9347004B2 (en) * | 2009-06-16 | 2016-05-24 | The Boeing Company | Flame propagation resistant foam and method |
| CN102504173B (en) * | 2011-10-21 | 2013-12-18 | 上海摩尔舒企业发展有限公司 | Shape memory spraying polyurethaneurea elastomer resin bathroom product and preparation method thereof |
| US9587139B2 (en) | 2012-06-15 | 2017-03-07 | 3M Innovative Properties Company | Curable polyurea forming composition, method of making, and composite article |
| ITTV20120242A1 (en) * | 2012-12-21 | 2014-06-22 | Mas Gianluigi Dal | BUILT-IN LIGHTING DEVICE AND ITS PRODUCTION METHOD |
| CN103304761B (en) * | 2013-05-27 | 2015-03-25 | 广州市台实防水补强有限公司 | Polyurea and preparation method thereof |
| CN103709924A (en) * | 2013-12-30 | 2014-04-09 | 刘太安 | Spraying quick-drying heat-insulating waterproof paint and production method thereof |
| CN105505159A (en) * | 2015-12-04 | 2016-04-20 | 大连怿文新材料科技发展有限公司 | Rapidly cured rigid polyurea with high adhesion and preparation method of rapidly cured rigid polyurea |
| CN105384888B (en) * | 2015-12-21 | 2017-12-26 | 青岛理工大学 | Viscoelastic damping material with good conductivity and preparation method thereof |
| CN109439159A (en) * | 2018-11-07 | 2019-03-08 | 惠州市祯华化工有限公司 | A kind of spray polyurea material and spray polyurea plate of material, preparation method |
| CN110117381B (en) * | 2019-05-10 | 2022-03-11 | 汇星海科技（天津）有限公司 | EPO foam material surface hardening treatment process and application |
| CN110804155A (en) * | 2019-11-06 | 2020-02-18 | 青岛爱尔家佳新材料股份有限公司 | Flame-retardant spray polyurea material and preparation method thereof |
| CN111363120A (en) * | 2020-04-24 | 2020-07-03 | 长沙盾甲新材料科技有限公司 | High-strength spraying polyurethane material containing reactive flame retardant and preparation method thereof |
| CN111518462A (en) * | 2020-05-28 | 2020-08-11 | 胜利油田新大管业科技发展有限责任公司 | Anticorrosive spray polyurea elastomer and preparation method and application thereof |
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